WO2017194380A1 - Procédé pour la préparation d'une masse de moulage thermoplastique - Google Patents

Procédé pour la préparation d'une masse de moulage thermoplastique Download PDF

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Publication number
WO2017194380A1
WO2017194380A1 PCT/EP2017/060619 EP2017060619W WO2017194380A1 WO 2017194380 A1 WO2017194380 A1 WO 2017194380A1 EP 2017060619 W EP2017060619 W EP 2017060619W WO 2017194380 A1 WO2017194380 A1 WO 2017194380A1
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WO
WIPO (PCT)
Prior art keywords
section
thermoplastic molding
mixing
housing
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2017/060619
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German (de)
English (en)
Inventor
Wolfgang Fischer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ineos Styrolution Group GmbH
Original Assignee
Ineos Styrolution Group GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ineos Styrolution Group GmbH filed Critical Ineos Styrolution Group GmbH
Priority to US16/099,710 priority Critical patent/US10710274B2/en
Priority to MX2018013595A priority patent/MX2018013595A/es
Priority to EP17720168.8A priority patent/EP3455043B1/fr
Priority to ES17720168T priority patent/ES2829292T3/es
Priority to KR1020187035550A priority patent/KR102311444B1/ko
Publication of WO2017194380A1 publication Critical patent/WO2017194380A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B29B7/488—Parts, e.g. casings, sealings; Accessories, e.g. flow controlling or throttling devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/82—Heating or cooling
    • B29B7/823—Temperature control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/84—Venting or degassing ; Removing liquids, e.g. by evaporating components
    • B29B7/842—Removing liquids in liquid form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/84—Venting or degassing ; Removing liquids, e.g. by evaporating components
    • B29B7/845—Venting, degassing or removing evaporated components in devices with rotary stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/256—Exchangeable extruder parts
    • B29C48/2565—Barrel parts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/76—Venting, drying means; Degassing means
    • B29C48/762—Vapour stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/76—Venting, drying means; Degassing means
    • B29C48/765—Venting, drying means; Degassing means in the extruder apparatus
    • B29C48/766—Venting, drying means; Degassing means in the extruder apparatus in screw extruders
    • B29C48/767—Venting, drying means; Degassing means in the extruder apparatus in screw extruders through a degassing opening of a barrel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/80—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the plasticising zone, e.g. by heating cylinders
    • B29C48/82—Cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/80—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the plasticising zone, e.g. by heating cylinders
    • B29C48/83—Heating or cooling the cylinders
    • B29C48/834—Cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/005—Processes for mixing polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/203—Solid polymers with solid and/or liquid additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02—Homopolymers or copolymers of hydrocarbons
    • C08L25/04—Homopolymers or copolymers of styrene
    • C08L25/08—Copolymers of styrene
    • C08L25/12—Copolymers of styrene with unsaturated nitriles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/18—Homopolymers or copolymers of nitriles
    • C08L33/20—Homopolymers or copolymers of acrylonitrile
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B29B9/065—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion under-water, e.g. underwater pelletizers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/285—Feeding the extrusion material to the extruder
    • B29C48/29—Feeding the extrusion material to the extruder in liquid form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2009/00—Use of rubber derived from conjugated dienes, as moulding material
    • B29K2009/06—SB polymers, i.e. butadiene-styrene polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2021/00—Use of unspecified rubbers as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2021/00—Use of unspecified rubbers as moulding material
    • B29K2021/003—Thermoplastic elastomers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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    • C08J2325/04—Homopolymers or copolymers of styrene
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    • C08J2325/12—Copolymers of styrene with unsaturated nitriles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2333/08—Homopolymers or copolymers of acrylic acid esters

Definitions

  • thermoplastic molding composition
  • the present invention relates to a process for producing a thermoplastic molding composition by means of an extruder, the extruder comprising an introduction zone, a mixing section, a degassing section and a discharge zone.
  • a water-containing first component of the thermoplastic molding composition and a second component of the thermoplastic molding compound are fed, mixed in the mixing section, the thermoplastic molding material and evaporated water evaporated in the degassing water vapor is removed from the thermoplastic molding material, and in the discharge zone the thermoplastic molding compound is discharged.
  • the present invention furthermore relates to a thermoplastic molding compound produced by the process according to the invention and also to moldings.
  • thermoplastic (co) polymers such as acrylonitrile-butadiene-styrene (ABS) or acrylonitrile-styrene-acrylate (ASA)
  • ABS acrylonitrile-butadiene-styrene
  • ASA acrylonitrile-styrene-acrylate
  • the educts, in particular styrene-acrylonitrile copolymer (SAN) and polybutadiene, or acrylate rubber are fed to an extruder. Within the extruder, melting and mixing or dispersion of the educts into a molding compound or a polymer blend takes place.
  • the supplied polybutadiene, or the acrylate rubber is dispersed in a styrene-acrylonitrile matrix.
  • a twin-screw extruder for extruding molding compositions is known.
  • the twin-screw extruder comprises two screws, which are accommodated in a housing, and which rotate in the same direction.
  • the twin-screw extruder further comprises a feed zone, a conversion zone and a discharge zone.
  • the educts are fed to the feed zone, which has a feed opening for this purpose.
  • the educts can be melted in solid form, in particular as granules, but also melted and thus fed viscous the feed zone.
  • the educts are taken up in the feed zone by means of the two screws, further promoted and compacted.
  • a melting and homogenizing of the molding material takes place in the conversion zone.
  • a further homogenization of the molten mass is carried out in the discharge zone. If appropriate, remaining residues of solid particles are still melted. Furthermore, there is a uniform distribution of the substance components.
  • the temperature of the melt is also standardized. Furthermore, a pressure required for granulation is built up in the discharge zone.
  • WO 1998/13412 describes screw machines which have at least one squeezing section with at least one damming element and an associated dewatering opening upstream of the first damming element.
  • the screw machines contain degassing sections that lie after the last plastication section.
  • the vent openings and drainage openings may be provided with a device which prevents the escape of extruded material. Retaining screws are described as preferred for this purpose.
  • EP-A 0735077 describes the production of impact-modified thermoplastics by mechanical dewatering of an elastomeric component and mixing with a thermoplastic polymer in a screw machine.
  • the drainage holes are provided with retaining screws and are operated under pressure.
  • JP S02-286208 (1990) three different dewatering processes are disclosed by means of an extruder equipped with two screws.
  • the extrusion composition is in each case withdrawn moisture in liquid form and additionally in gaseous form via strainer housing.
  • JP H57-167303 (1982) describes that an extrusion mass, in this case e.g. Slurry of polymer particles, dosed into a twin-screw extruder, dehydrated, degassed and kneaded. Upstream of the compression zone, water in liquid form may exit the extruder. Residual moisture can escape in gaseous form. As drainage openings strainer housings are used.
  • JP H60-222223 (1985) discloses a method in which an extruded material, preferably a food but also other materials, water is removed in liquid form. The drainage is carried out by means of a twin-screw extruder. Discharge of the moisture takes place backwards through an opening which is connected to a vacuum pump.
  • WO 2004/028781 discloses a device for extruding thermoplastics, in particular a screw machine.
  • the device in this case comprises a degassing opening and a drainage opening, which is equipped for example with a metal wire mesh.
  • a generic method for the production of thermoplastic molding compositions by means of an extruder is known.
  • the extruder comprises, inter alia, a metering section in which a rubber containing water is supplied, a squeeze section in which the rubber is partially dehydrated, and a feed section in which a styrene-acrylonitrile copolymer (SAN) is supplied.
  • SAN styrene-acrylonitrile copolymer
  • the rubber and styrene-acrylonitrile copolymer (SAN) are then blended into the thermoplastic molding compound.
  • the extruder further includes a plastication section or mixing section in which the thermoplastic molding compound is mixed, thereby evaporating contained water, a degassing section in which water vapor is removed from the thermoplastic molding compound, and a discharge zone in which the thermoplastic molding compound is discharged. Inside the extruder, an extruder screw rotates.
  • thermoplastic molding compound within the extruder in particular within the mixing section, has a temperature of for example 220-240 ° C, e.g. 230 ° C. This temperature is achieved mainly by a heat input by introduced by the rotating extruder screw mechanical energy. In addition, it is customary to heat housing of the extruder from the outside.
  • the incorporated rubber may contain salts dissolved in the contained water. When evaporating the water thus salt particles of different sizes. The evaporation of the water takes place inter alia in the mixing section.
  • the larger salt particles can then at least partially block holes in a perforated plate or nozzle bar in the discharge zone.
  • a diameter of a discharged thread is reduced. If the diameter of the discharged thread is reduced too much, the thread may break.
  • a diameter of the discharged thermoplastic molding compound is also reduced. After cutting granules thus result in reduced volume and reduced mass. Such a reduced granule is also called undersize.
  • thermoplastic molding composition If relatively large salt particles pass through the holes of the perforated plate in the discharge zone, then they are later contained in the discharged granulated thermoplastic molding composition and visible as surface defects, especially when the thermoplastic molding composition continues to thin films is processed. On contact with warm water, the smaller salt particles can then swell and form salt specks, which are also visible in the form of surface defects on the thermoplastic molding compound. It is an object of the invention to reduce clogging of holes in a perforated plate in the discharge zone of an extruder and to avoid the formation of salt spots in the discharged (granulated) thermoplastic molding compound. This object is achieved by a method for producing a thermoplastic molding composition by means of an extruder with the features of claim 1.
  • thermoplastic molding materials and thermoplastics have been known to the skilled person for years, such as e.g. Polyamides, polycarbonates, styrene polymers, styrene copolymers or mixtures of these polymers.
  • the styrene copolymers include, for example, styrene / acrylonitrile copolymers (SAN), rubber-modified styrene copolymers such as acrylonitrile-butadiene-styrene (ABS) and acrylonitrile-styrene-acrylate (ASA).
  • SAN styrene / acrylonitrile copolymers
  • ABS acrylonitrile-butadiene-styrene
  • ASA acrylonitrile-styrene-acrylate
  • an extruder which comprises at least one entry zone, at least one mixing section, at least one degassing section and at least one discharge zone.
  • a water-containing first component of the thermoplastic molding composition and a second component of the thermoplastic molding material are supplied in the at least one entry zone, in the at least one mixing section, the thermoplastic molding compound is mixed and water is evaporated, in the at least one degassing is water vapor from the thermoplastic Removed molding compound, and in the at least one discharge zone, the thermoplastic molding material is discharged.
  • the discharge zone has, for example, a perforated plate through whose holes the thermoplastic molding compound is discharged.
  • At least one of the mixing housings of the mixing section is maintained at a temperature equal to or lower than a temperature of the thermoplastic molding compound within the mixing section.
  • the mixing housings of the mixing section are kept completely at a temperature equal to or lower than a temperature of the thermoplastic molding compound within the mixing section.
  • the mixing housing of the mixing section may be kept at the same or lower temperature, for example, by omitting active heating of the mixing housing of the mixing section.
  • the mixing housing can therefore be operated adiabatically. But also an active cooling of the mixing housing of the mixing section by means of air cooling or liquid cooling is conceivable.
  • the temperature at which at least one of the mixing housings of the mixing section is maintained is at least 10 K lower than the temperature of the thermoplastic molding compound within the mixing section.
  • the temperature at which at least one of the mixing housings of the mixing section is maintained is at least 20 K lower than the temperature of the thermoplastic molding compound within the mixing section.
  • At least one housing of the degassing section is heated such that a temperature of the housing of the degassing section is higher than the temperature of at least one mixing housing of the mixing section.
  • At least one housing of the discharge zone is heated such that a temperature of the housing of the Discharge zone is higher than the temperature of at least one mixing housing of the mixing section.
  • At least one housing of the entry zone is heated such that a temperature of the housing of the entry zone is higher than the temperature of at least one mixing housing of the mixing section.
  • the water-containing first component of the thermoplastic molding composition and the second component of the thermoplastic molding composition can be supplied to the extruder together in the entry zone according to a possible embodiment of the invention.
  • the at least one entry zone of the extruder comprises at least one dosing section, at least one squeeze section and at least one feed section.
  • a water-containing first component of the thermoplastic molding composition is supplied in the at least one metering, in the at least one Abquetschab songs the first component of the thermoplastic molding composition is partially dehydrated, and in the at least one feed section, a second component of the thermoplastic molding material is supplied.
  • At least one housing of the feed section is heated such that a temperature of the housing of the feed section is higher than the temperature of at least one mixing housing of the mixing section.
  • the first component of the thermoplastic molding compound fed into the metering section of the feed zone of the extruder is preferably an elastomer.
  • any polymer which has elastomeric properties and can be fed to an extruder can be used as the elastomer. It can also be used a mixture of different elastomers.
  • elastomers are polymers of conjugated dienes, such as butadiene, with a vinyl aromatic compound-based outer graft, such as SAN copolymers.
  • graft rubbers based on crosslinked polymers of C1-C12-alkyl esters of acrylic acid such as n-butyl acrylate, ethylhexyl acrylate, grafted with polymers based on vinylaromatic compounds such as SAN copolymers.
  • Graft rubbers which essentially contain a copolymer of conjugated dienes and C 1 -C 12 -alkyl acrylates, for example a butadiene-n-butyl acrylate copolymer, and an outer grafting stage of SAN copolymer, polystyrene or PMMA are also generally used.
  • the preparation of such graft rubbers by the customary processes, in particular by emulsion or suspension polymerization, is known.
  • the first component of the thermoplastic molding compound fed into the metering section of the feed zone of the extruder is a rubber.
  • the rubber is in particulate form.
  • Particularly preferred are those rubbers which have a grafted shell of other, usually non-elastomeric polymers.
  • the graft rubber types fed to the extruder as partially dewatered material contain up to 50% by weight, particularly preferably 25% by weight to 40% by weight, of residual water.
  • two-stage or multi-stage graft rubbers in which the elastomeric base or graft stages are polymerized by polymerization of one or more of the monomers butadiene, isoprene, chloroprene, styrene, alkylstyrene, C1- to C12-alkyl esters of acrylic acid or methacrylic acid and lower Amounts of other, even crosslinking monomers can be obtained, and in which the hard grafting stages of one or more of the monomers styrene, alkylstyrene, acrylonitrile, methyl methacrylate are polymerized.
  • up to 10% by weight of functional groups bearing, polar monomers or crosslinking monomers may be copolymerized.
  • ABS acrylonitrile-butadiene-styrene
  • a rubber is fed into the metering section of the entry zone of the extruder, the rubber containing polybutadiene.
  • a SAN-grafted polybutadiene can be used.
  • ASA acrylonitrile-styrene-acrylate
  • ASA acrylonitrile-styrene-acrylate
  • an acrylate eg butyl acrylate component
  • a SAN-grafted alkyl acrylate can also be used, for example.
  • the second component of the thermoplastic molding compound fed into the feed section of the feed zone of the extruder is preferably a thermoplastic polymer (as a matrix) such as styrene-acrylonitrile copolymer (SAN), polystyrene, polymethyl methacrylate, polyvinyl chloride, polyamide (e.g. Terblend®) or mixtures of these polymers.
  • SAN styrene-acrylonitrile copolymer
  • polystyrene polystyrene
  • polymethyl methacrylate polyvinyl chloride
  • polyamide e.g. Terblend®
  • thermoplastic polymers are also polycarbonates, polyalkylene terephthalates such as polybutylene terephthalate and polyethylene terephthalate, polyoxymethylene, polymethyl methacrylate, polyphenylene sulfide, polysulfones, polyethersulfones and polyamides, and mixtures of these thermoplastics.
  • thermoplastic elastomers such as thermoplastic polyurethane (TPU) can also be used.
  • copolymers based on styrene / maleic anhydride, styrene / imidated maleic anhydride, styrene / maleic anhydride / imidated maleic anhydride, styrene / methyl methacrylate / imidated maleic anhydride, styrene / methyl methacrylate, styrene / methyl methacrylate / maleic anhydride, methyl methacrylate / imidated maleic anhydride can be used as the second component , Styrene / imidated methyl methacrylate, imidated PMMA or mixtures of these polymers.
  • the styrene may be wholly or partly replaced by alpha-methylstyrene, or by nuclear-alkylated styrenes, or by acrylonitrile.
  • thermoplastic polymers are in particular those based on alpha-methylstyrene / acrylonitrile, styrene / maleic anhydride, styrene / methyl methacrylate and copolymers with imidêtm maleic anhydride.
  • the second component of the thermoplastic molding compound fed into the feed section of the feed zone of the extruder is a styrene-acrylonitrile copolymer (SAN).
  • SAN styrene-acrylonitrile copolymer
  • the second component is fed in the feed section of the entry zone of the extruder as a melt.
  • thermoplastic polymers which can be used as the second component, prepared by continuous bulk or solution polymerization, wherein the resulting melt, optionally after removal of the solvent, for example, with a melt pump continuously fed directly to the feed section of the entry zone of the extruder.
  • production by emulsion, suspension or precipitation polymerization is also possible, the polymer being separated from the liquid phase in an additional working step. Details of the preparation processes are described, for example, in Kunststoffhandbuch, Mr. R. Vieweg and G. Daumiller, Vol. V, "Polystyrene", Carl-Hanser-Verlag, Kunststoff, 1969, pp. 1 to p.
  • thermoplastic molding composition which causes no significant blockage of the holes the perforated plate during discharge from the discharge zone of the extruder, and has no visible on their surface salt pebbles.
  • the invention also relates to the molding compositions, moldings and a device for carrying out the method.
  • FIG. 1 a schematic sectional view of an extruder.
  • An extruder 10 shown schematically in FIG. 1 is in the present case designed as a twin-screw extruder.
  • the extruder 10 has two extruder screws, which rotate about parallel axes of rotation.
  • the two extruder screws are arranged within an elongated housing of the extruder 10.
  • the extruder 10 is used for the production of thermoplastic molding compositions, in particular acrylonitrile-butadiene-styrene (ABS) or acrylonitrile-styrene-acrylate (ASA).
  • ABS acrylonitrile-butadiene-styrene
  • ASA acrylonitrile-styrene-acrylate
  • the extruder 10 When viewed downstream, the extruder 10 has a metering section 22, a squeeze section 24, a feed section 26, a mixing section 30, a degassing section 40 and a discharge zone 50.
  • the individual sections and zones of the extruder 10 in this case have housings which are connected to one another by means of flanges.
  • the dosing section 22 of the extruder 10 serves to supply a water-containing first component of the thermoplastic molding composition to be produced.
  • the squeezing section 24 of the extruder 10 serves for partial dewatering of the first component of the thermoplastic molding compound.
  • the feed section 26 of the extruder 10 serves to supply a second component of the thermoplastic molding composition to be produced.
  • the squeezing section 24 is not absolutely necessary.
  • the dehydration can also take place, for example, in the mixing section 30.
  • the feed section 26 is not absolutely necessary.
  • the second component of the thermoplastic molding composition can also be fed to the extruder 10 together with the first component of the thermoplastic molding compound in the metering section 22.
  • the metering section 22, the squeezing section 24 and the feed section 26 together form a picking zone 20 of the extruder 10.
  • the picking zone 20 with the metering section 22 and the feed section 26 has two sections for feeding components of the thermoplastic molding compound to be produced.
  • the entry zone 20 has only such a section, which serves for supplying all components of the thermoplastic molding composition to be produced.
  • the entry zone 20 of the extruder 10 thus serves to supply the water-containing thermoplastic molding material.
  • the mixing section 30 of the extruder 10 serves to mix the thermoplastic molding composition. During the mixing, water contained in the thermoplastic molding material is also vaporized.
  • the degassing section 40 of the extruder 10 has a degassing opening, through which water vapor can escape and is thus removed from the thermoplastic molding compound.
  • the discharge zone 50 of the extruder 10 serves to discharge the thermoplastic molding compound from the extruder 10.
  • the discharge zone 50 has a perforated plate 60 which is provided with a plurality of holes. During the discharge from the discharge zone 50, the thermoplastic molding compound is pressed through the holes of the perforated plate 60.
  • a nozzle bar may also be provided on the discharge zone 50.
  • the metering section 22, the squeezing section 24, the feed section 26, the mixing section 30, the degassing section 40 and the discharge zone 50 each have housings which can be tempered, in particular heated, by means of external tempering devices, not shown here.
  • the said external devices may be electrically operated heating devices or else heating devices through which a liquid flows, as well as cooling devices.
  • the mixing section 30 in the present case has a first mixing housing 31 and a second mixing housing 32.
  • the first mixing housing 31 of the mixing section 30 is located upstream and adjoins the feed section 26.
  • the second mixing housing 32 of the mixing section 30 is located downstream and adjoins the degassing section 40.
  • the individual external temperature control are independently operable.
  • the housings of individual sections or zones of the extruder 10 can be heated or cooled in a targeted manner, while at the same time a tempering of housings of other sections or zones of the extruder 10 is omitted.
  • the first mixing housing 31 and the second mixing housing 32 of the mixing section 30 are independently temperature-controlled.
  • the first component of the thermoplastic molding composition that contains water is introduced into the metering section 22 of the extruder 10.
  • the first component is a particulate rubber which has a water content of from 1 to 40, preferably from 20 to 35, in particular about 30% by weight.
  • the rubber introduced into the metering section 22 is transported by the twin screw of the extruder 10 into the pinching section 24. In the squeezing section 24, partial dehydration of the rubber takes place.
  • the housing of the pinching section 24 is tempered by means of the tempering device, not shown, in particular cooled.
  • the second component of the thermoplastic molding composition to be produced is introduced.
  • the second component in the present case is styrene-acrylonitrile copolymer (SAN).
  • SAN styrene-acrylonitrile copolymer
  • the housing of the Zuurerabitess 26 is heated by means of the heater, not shown.
  • the rubber is transported from the twin screw of the extruder 10 from the squeezing section 24 into the feed section 26 and mixed with the imported into the feed section 26 styrene-acrylonitrile copolymer (SAN) to the thermoplastic molding compound.
  • the thermoplastic molding compound is transported from the twin screw of the extruder 10 from the feeding section 26 further into the mixing section 30. In the mixing section 30 of the extruder 10, a further thorough mixing of the thermoplastic molding compound takes place.
  • thermoplastic molding compound within the mixing section 30 has a measured temperature of about 230 ° C.
  • water which is still contained in the thermoplastic molding compound is evaporated.
  • the water vapor produced by the evaporation leaves the extruder 10 through a degassing opening provided in the degassing section 40.
  • the water vapor resulting from the evaporation is removed from the thermoplastic molding compound.
  • thermoplastic molding compound is transported by the twin screw of the extruder 10 from the mixing section 30 further into the degassing section 40, in which the resulting water vapor exits the extruder 10 through the degassing opening.
  • thermoplastic molding compound is transported by the twin screw of the extruder 10 further to the discharge zone 50.
  • the thermoplastic molding compound is discharged from the extruder 10.
  • the thermoplastic molding compound is pressed out of the extruder 10 through the holes in the perforated plate 60.
  • thermoplastic molding compound discharged from the extruder 10 is then granulated in a granulating unit not shown here.
  • the granulation takes place as underwater granulation.
  • emerging from the holes 60 of the perforated plate 50 threads are cut by means of a rotating knife to a predetermined length.
  • the knife and the emerging threads are in a water chamber. After cutting thus arise Granules.
  • a strand granulation in a water bath is feasible.
  • the first mixing housing 31 and the second mixing housing 32 of the mixing section 30 are heated to a temperature of about 240 ° C. This results in an average life of 15 days.
  • the service life is the time during which the extruder 10 produces the thermoplastic molding compound without interruption.
  • the service life ends here, when the holes in the perforated plate 60 or the holes in the nozzle bar of the extruder 10 are partially or completely blocked, and the perforated plate 60 or the nozzle bar must be cleaned.
  • the first mixing housing 31 of the mixing section 30 is heated to a temperature of about 240 ° C.
  • the second mixing housing 32 is operated adiabatically. This results in a service life of about 30 days.
  • the second mixing housing 32 of the mixing section 30 is heated to a temperature of about 240 ° C.
  • the first mixing housing 31 is operated adiabatically. It also results in a service life of 30 days.
  • the first mixing housing 31 and the second mixing housing 32 of the mixing section 30 are adiabatically operated. This results in a life of 40 days.
  • the first mixing housing 31 of the mixing section 30 is heated to a temperature of approximately 200 ° C.
  • the second mixing housing 32 is also heated to a temperature of about 200 ° C. This results in a service life of 45 days.
  • the first mixing housing 31 of the mixing section 30 is heated to a temperature of approximately 200 ° C.
  • the second mixing housing 32 is heated to a temperature of about 240 ° C. This results in a life of 40 days.

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  • Mechanical Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

L'invention concerne un procédé pour la préparation d'une masse de moulage thermoplastique au moyen d'une extrudeuse (10), qui comprend au moins une zone d'introduction (20), au moins une section de mélange (30), au moins une section de dégazage (40) et au moins une zone de sortie (50), un premier composant contenant de l'eau ainsi qu'un deuxième composant étant introduits dans ladite au moins une zone d'introduction (20), la masse de moulage thermoplastique étant mélangée et l'eau contenue étant évaporée dans ladite au moins une section de mélange (30), la vapeur d'eau étant éliminée de la masse de moulage dans ladite au moins une section de dégazage (40) et la masse de moulage étant évacuée dans ladite au moins une zone d'évacuation (50). Ce faisant, au moins un des carters de mélange (31, 32) est maintenu à une température qui est égale ou inférieure à la température de la masse de moulage à l'intérieur de la section de mélange (30).
PCT/EP2017/060619 2016-05-10 2017-05-04 Procédé pour la préparation d'une masse de moulage thermoplastique Ceased WO2017194380A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US16/099,710 US10710274B2 (en) 2016-05-10 2017-05-04 Method for producing a thermoplastic moulding compound
MX2018013595A MX2018013595A (es) 2016-05-10 2017-05-04 Metodo para producir un compuesto de moldeo termoplastico.
EP17720168.8A EP3455043B1 (fr) 2016-05-10 2017-05-04 Procédé pour la préparation d'une masse de moulage thermoplastique
ES17720168T ES2829292T3 (es) 2016-05-10 2017-05-04 Procedimiento para la fabricación de una masa termoplástica de moldeo
KR1020187035550A KR102311444B1 (ko) 2016-05-10 2017-05-04 열가소성 몰딩 화합물의 제조 방법

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EP16168844 2016-05-10
EP16168844.5 2016-05-10

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WO2017194380A1 true WO2017194380A1 (fr) 2017-11-16

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JPS57167303A (en) 1981-04-08 1982-10-15 Toshiba Mach Co Ltd Recovery of polymer from undried polymer bead or polymer slurry
JPS60222223A (ja) 1984-04-19 1985-11-06 Ikegai Corp 押出機における供給素材の脱液方法及びその装置
JPH02286208A (ja) 1989-04-27 1990-11-26 Toshiba Mach Co Ltd 熱可塑性樹脂の脱水・乾燥成形用二軸押出機
EP0490056A1 (fr) * 1990-12-14 1992-06-17 HERMANN BERSTORFF Maschinenbau GmbH Procédé et dispositif pour la fabrication continue et directe d'un mélange à base de caoutchouc et d'un mélange fini de caoutchouc pour pneumatiques de véhicules, pour courroies de transmission, pour bandes de transport ainsi que pour des articles techniques en caoutchouc dans un seule installation de mélange
EP0735077A1 (fr) 1995-03-27 1996-10-02 BASF Aktiengesellschaft Procédé de préparation de thermoplastes
WO1998013412A1 (fr) 1996-09-26 1998-04-02 Basf Aktiengesellschaft Procede de production de thermoplastiques
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WO2009103714A2 (fr) 2008-02-19 2009-08-27 Basf Se Dispositif d'extrusion de masses à mouler
WO2015004112A1 (fr) 2013-07-11 2015-01-15 Styrolution Group Gmbh Procédé pour réaliser des matieres a mouler thermoplastiques et matieres a mouler thermoplastiques ainsi réalisées

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JPS57167303A (en) 1981-04-08 1982-10-15 Toshiba Mach Co Ltd Recovery of polymer from undried polymer bead or polymer slurry
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JPH02286208A (ja) 1989-04-27 1990-11-26 Toshiba Mach Co Ltd 熱可塑性樹脂の脱水・乾燥成形用二軸押出機
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WO2015004112A1 (fr) 2013-07-11 2015-01-15 Styrolution Group Gmbh Procédé pour réaliser des matieres a mouler thermoplastiques et matieres a mouler thermoplastiques ainsi réalisées

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EP3455043A1 (fr) 2019-03-20
KR20190006184A (ko) 2019-01-17
US20190193302A1 (en) 2019-06-27
EP3455043B1 (fr) 2020-09-30
MX2018013595A (es) 2019-06-03
US10710274B2 (en) 2020-07-14
KR102311444B1 (ko) 2021-10-15

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